Process of making metallic catalyzers.



i UNITED STATES PATENT OFFICE.

EIJWIN CUNO KAYSER, OF CINCINNATI, OHIO, ASSIGNOR TO THE PROCTER &GAMBLE COMPANY, OF CINCINNATI, OHIO, A CORPORATION OF OHIO.

PROCESS OF -MAKING METALLIC CATALYZEBS.

No Drawing.

Specification of Letters Patent. Application ,flled January 10, 1908.Serial No. 410,036.

Patented Sept. 26, 1911.

and useful Improvements in Metallic Catalyzers and Methods of Preparingthe Same, of which the following is a specification.

Following the observations of Sabatier, Senderens and others, finelydivided metals, exercising catalytic action and accordingly described ascatalyzers have of late been occasionally employed to induce chemicalreactions, whereof'many can not be brought about by any other means. Forinstance, it is known that by intervention of such catalyzersunsaturated fatty acids or their a v glycerids may be inade to absorbgaseous hydrogen, whereby they become converted into the correspondingsaturated compounds and thus hardened,

There arevarious known ways for pro ducing metallic powders in a stateof fine division- Nickel-powder,-which for many purposes is recognizedas the most potent catalyzer technically available, is, for example,most conveniently produced by acting upon such nickel compounds as thechlorid, oxid, hydrate .or carbonate at an adequate temperature with areducin gas,

' like hydrogen. The catalytic energy 0 such a powder, however carefullyrepared, is at best an uncertain quantity; gequently it is feeble, andsometimes, for no conclusive reason, it is altogether lacking.Furthermore, powder thus produced is specifically heavy and not easilykept in suspension in a liquid medium like oil, when that isdesired, norcan it, since it forms an almost impervious sediment, be readilyseparated and recovered from such liquid medium by a contrivance likethe filter-press. The same objections apply to nickelowder pre ared byother means. Altoget er, the di culties. of preparing reliablecatalyzers, and nickel catalyzers in particular, are well recognized andhave largel prevented such catalyzers from gaining in ustrialimportance.

Now, the object of my invention is to provide a method for producingcatalyzers of a reliable and uniform degree of activity and, inproportion to the quantity of metal employed, of higher' efliciency thanthe best metallic catalyzers hitherto obtained, and to .tion ofcarbonate or produce on an industrial scale metalliferous substances,possessing these qualities, convenient and economical for and in use,and which can be dealt with as an article of commerce.

I have discovered that by bringing suitable soluble or insoluble comounds of nickel, such as the nitrate, oxid, liydrate or carbonate, in anappropriate manner, into intimate combination with an inert, absorgtiveand comparatively bul mineral su stance, such as kieselguhr-in sorialearthdrying and comminuting the roduct, and reducing the powder thus prouced, highly eflicient and reliable catalyzers may at all timesbeproduced. These catalyzers have 'moreover a comparatively low specificgravity, so that they can at 'will be kept readily suspended in a liquidmedium such as oil; 1 they also possess the great technical advantage offorming an excellent filter-bed, and may in conse uence be rapidly andcompletely recovered rom the oil or other liquid,

wherein they may have been suspended durin use, by means of thefilterpress.

ne specific method of carrying out my invention is, to permeate orsaturate kieselguhr or other inert, absorptive, refractory 2 materialwitha solution of nickel-nitrate, dry the mixture, employingin the caseof the nitrate sufiicient heat to expel the nitric acid, grind orotherwise comminute the resulting product, and reduce with hydrogen.

Another method is, -to permeate or saturate kieselguhr or other inert,absorptive,

refractory material with a solution of nickelchlorid, nickel-sulfate orother soluble nickelsalt, enter the resulting product, with or deredcarbonate of soda or other suitable powdered precipitant, throw themixture with constant stirring into boiling water,

. dry and comminute the mixture, and reduce as before.

To develop the highest catalytic efliciency,

the kieselguhr should become evenly and completely coated andpermeated-plated with a film of metal. Above and below this point ofcomplete and even metallization beneficial results may still be secured,but the full benefit of my process and the economy derived therefromwill not be realized.

I do not limit myself to any particular proportion as between nickel andkieselguhr,

the less so as there are on the market many varieties of. kieselguhr ofdiverse specific gravity and absorptive power and as the ultimate objectof the catalyzer may have to be taken into account. A catalyzer,composed of one to two parts by weight of metallic nickel and four partsby weight of kieselguhr has however proved very efiective in saturatingfats and oils by meansof hydrogen.

I claim as my invention:

1. The method of preparing a catalyzer, consisting in diffusing asolution of a reducible nickel-oxygemsalt over and through kieselguhr,drying and comminuting the product, and reducing the powder withhydrogen. V

2. The method of producing a catalyzer, consisting in precipitating a:reducible, insoluble nickel compound within and upon an inert,absorptive and comparatively bulky mineral substance; removing thesoluble salts formed during precipitation by washing; then drying theproduct; and reducing.

the powder with hydrogen.

3. The method of producing a catalyzer,

consisting in precipitating a reducible, insoluble nickel compoundwithin and upon an inert, absorptive andcomparatively bulky mineralsubstance; removing the soluble salts formed during precipitation bywashing; then drying and comminuting the product; and reducing thepowder with hydrying and comminuting the product; and reducing thepowder wit-h hydrogen.

5. The methodof preparing a metalliferous catalyzer, whlch consists inconvertmg by. a process of precipitation a soluble nickel-salt,intimately incorporated with a refractory inert material, into aninsoluble compound, removing all soluble products of reaction, dryingand comminuting the residue and submitting it to the reducing action ofhydrogen. n

6. The method of preparing a metalliferous' catalyzer, which consists inpermeating a refractory inert material with an absorbable proportion ofan aqueous solution of a nickel-salt, then incorporating therewith amolecular proportion of a dry pulverous precipitant, then boiling themixture with water and removing all soluble products formed, drying andcomminuting the residue and submitting it to the reducing action ofhydrogen.

7. The method of preparing a metallife'rous catalyzer, which consists inboiling a refracw inert material permeated with a water-solublenickel-salt in water containing a nickel-precipitant, removing allsoluble products of reaction, drying and comminuting the residue'andsubmitting it to the reducing action of hydrogen.

EDWIN CUNO 'KAYSER.

Witnesses:

E. LA Coon, W. W. SYMMES.

